Labconco 7934040 User-Service Manual PDF

User’s Manual
FreeZone® 6, 12 and 18 Liter

Freeze Dry Systems
Models
7753020 7753522 7754030 7755030 7934020 7960030
7753021 7753524 7754031 7755031 7934021 7960031
7753022 7753532 7754032 7755032 7934022 7960032
7753024 7753534 7754034 7755034 7934024 7960034
7753026 7753542 7754036 7755036 7934026 7960036
7753027 7753544 7754037 7755037 7934027 7960037
7753030 7754040 7755040 7934030 7960040
7753031 7754041 7755041 7934031 7960041
7753032 7754042 7755042 7934032 7960042
7753034 7754044 7755044 7934034 7960044
7753036 7754046 7755046 7934036 7960046
7753037 7754047 7755047 7934037 7960047
7753040 7934040
7753041 7934041
7753042 7934042
7753044 7934044
7753046 7934046
7753047 7934047
Labconco’s Mascot,
Labby the LABster
FreeZone® is a registered trademark of Labconco Corporation.
Warranty
Labconco provides a warranty on all parts and factory workmanship. The warranty includes areas of
defective material and workmanship, provided such defect results from normal and proper use of the
equipment.
The warranty for all Labconco products will expire one year from date of installation or two years from
date of shipment from Labconco, whichever is sooner, except the following:
• Purifier® Delta® Series Biological Safety Cabinets and PuriCare® Lab Animal Products carry a
three-year warranty from date of installation or four years from date of shipment from Labconco,
whichever is sooner.
• Steamscrubber & FlaskScrubber Glassware Washers carry a two year warranty from date of
installation or three years from date of shipment from Labconco, whichever is sooner.
• Carts carry a lifetime warranty.
• Glassware is not warranted from breakage when dropped or mishandled.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event of a
warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause is
determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all
defective parts to restore the unit to operation. Under no circumstances shall Labconco Corporation be
liable for indirect, consequential, or special damages of any kind. This statement may be altered by a
specific published amendment. No individual has authorization to alter the provisions of this warranty
policy or its amendments. Lamps and filters are not covered by this warranty. Damage due to corrosion or
accidental breakage is also not covered.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by
various federal, state, or local regulations. All users of this equipment are required to become familiar with
any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water,
land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to
user’s compliance with such regulations.
Part #7403400 Rev C

ECO C639
For more information, please contact us:
ExpotechUSA
10700 Rockley Road
Houston, Texas 77099
USA
281-496-0900 [voice]
281-496-0400 [fax]
E-mail: sales@expotechusa.com
Website: www.ExpotechUSA.com
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION 1
Freeze Dry Process 1
Freeze Dry Rates 2
Freeze Dry Capacity 3
Samples Containing Volatile Substances 4
About This Manual 4
Typographical Conventions 6
CHAPTER 2: PREREQUISITES 7
Electrical Requirements 7
Location Requirements 8
Vacuum Pump Requirements 8
Chamber or Manifold Requirements 8
CHAPTER 3: GETTING STARTED 9

Unpacking Your Freeze Dryer 9
Freeze Dryer Components 10
Setting Up Your Freeze Dryer 12
Vacuum Pump Connection 13
Electrical Connection 14
Drying Chamber or Drying Manifold Installation 14
Chemical Resistance of Freeze Dryer Components 14
Solvent Safety Precautions 16
CHAPTER 4: USING YOUR FREEZE DRYER 18

Freeze Dryer Controls 19
Operation Checklist 21
Vacuum Pump Ballast Setting 21
Purge Valve 21
Operating the Freeze Dryer 22
Set-Up 22
Baffle 25
Automatic Start-Up 25
Automatic Start Up with Purge Valve 25
Manual Start-Up 26
Manual Start-Up with Purge Valve 26
Setting the Operating Vacuum Level 27
Pre-Freezing Samples 27
Adding Sample 28
Shut Down 29
Defrosting 29
Operating the Shell Freezer 30
Operating the Vacuum Drying Chamber 31
Alarms 32
Power Failure 32
Line Voltage Out of Range 33
Temperature Out of Range 33
Service Vacuum Pump 34
Moisture in Collector 34
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 35
CHAPTER 6: USING THE RS232 RECEPTACLE 37

Computer Connection for Computer Interface 37
CHAPTER 7: TROUBLESHOOTING 42
Vacuum Pump 42
Gaskets, Tubing, Connections, Sample Valves 43
System Components & Collection Chamber Isolation 45
Refrigeration Module Operation 48
CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY 49

Temperature & Vacuum Display 49
Line Voltage Alarm Points 49
Moisture Sensor Alarm 50
Modifying the Display 50
APPENDIX A: FREEZE DRYER COMPONENTS 54
APPENDIX B: FREEZE DRYER DIMENSIONS 59
APPENDIX C: FREEZE DRYER SPECIFICATIONS 60

Electrical Specifications 60
Environmental Conditions 63
Wiring Diagrams 64
APPENDIX D: FREEZE DRYER ACCESSORIES 67
DECLARATION OF CONFORMITY 76
CHAPTER 1
INTRODUCTION
Congratulations on your purchase of a Labconco FreeZone®
Freeze Dry System, which is designed for laboratory lyophilization
procedures. The refrigerant used in the refrigeration system is
CFC-free so it will not endanger the environment. The unit is easy
to install and maintain. Proper care and maintenance of this
product will result in many years of dependable service.
Freeze Dry Process

Freeze drying is an important process in sample preparation and
for the preservation and storage of biologicals, pharmaceuticals
and foods. Of the various methods of dehydration, freeze drying
(lyophilization) is especially suited for substances that are heat
sensitive. Other than food processing (e.g., coffee, whole dinners),
freeze drying has been extensively used in the development of
pharmaceuticals (e.g., antibiotics) and preservation of biologicals
(e.g., proteins, plasma, viruses and cell lines). The nondestructive
nature of this process has been demonstrated by the retention of
viability in freeze dried viruses and microorganisms.
Freeze drying is a process whereby water or other solvent is

removed from frozen material by converting the frozen water
directly into vapor without the intermediate formation of liquid
water. The basis for this sublimation process involves the
absorption of heat by the frozen sample in order to vaporize the
ice; the use of a vacuum pump to enhance the removal of water
vapor from the surface of the sample; the transfer of water vapor to
a collector; and the removal of heat by the collector in order to
condense the water vapor. In essence, the freeze dry process is a
balance between the heat absorbed by the sample to vaporize the
1
Chapter 1: Introduction
ice and the heat removed from the collector to convert the water
vapor into ice.
Freeze Dry Rates

The efficiency of the freeze drying process is dependent upon the
surface area and the thickness of the sample, the collector
temperature and vacuum obtained, the eutectic point and solute
concentration of the sample. It is important to remember these
factors when trying to obtain efficient utilization of your freeze dry
system. A listing of selected materials and their approximate
drying times are shown in Table 1 for your reference.
Table 1
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material Safe Collector Hours
10mm Thick Temperature Temperature (Approx.)
°C °C
Milk -5 -40 10
Urea -7 -40 10
Blood Plasma -10 to -25 -40 16
Serum -25 -40 18
Vaccinia -30 to -40 -50 22
Influenza Vaccine -30 -50 24
Human Tissue -30 to -40 -50 48
Vegetable Tissue -50 -80 60
*Total sample quantities are contingent on various freeze dryer capacities.
Up to the point of overloading the system, the greater the surface

area of the sample, the faster the rate of freeze drying. By contrast,
for a given surface area, the thicker the sample the slower the rate
of freeze drying. This is based on the fact that the heat of
sublimation is usually absorbed on one side of the frozen sample
and must travel through the frozen layer to vaporize water at the
other surface. In addition, as the sample is freeze dried, the water
vapor must travel through the layer of dried material. The thicker
the sample, the greater the chance that the dried layer may collapse
which would cause an additional decrease in the rate of freeze
drying.
The surface area and thickness of the sample can usually be

ignored when each sample contains only a few milliliters.
However, for larger volumes, the samples should be shell frozen to
maximize the surface area and minimize the thickness of the
2
sample. The volume of the freeze dry flask should be two to three
times the volume of the sample.
In order for lyophilization to occur, ice must be removed from the

frozen sample via sublimation. This is accomplished by the
collector and the vacuum pump. The collector, which should be at
least 15 to 20°C colder than the eutectic temperature (melting
temperature) of the sample, traps vapor as ice. Since the vapor
pressure at the collector is lower than that of the sample, the flow
of water vapor is from the sample to the collector. Since this vapor
diffusion process occurs very slowly under normal atmospheric
conditions, a good vacuum is essential to maintain an efficient rate.
In many applications, the maintenance of a vacuum of 0.133 mBar
or less is recommended.
The rate of freeze drying is directly proportional to the vapor

pressure and the vapor pressure is dependent upon both eutectic
temperature and solute concentration of the sample. For example,
a solution of sodium chloride and water would freeze dry at a
slower rate than pure water. The eutectic temperature of a sodium
chloride solution is about –21°C and at this temperature the vapor
pressure is about 1/16 that of water at 0°C. Although the eutectic
temperature is not dependent upon the concentration of sodium
chloride, the vapor pressure of the water would decrease as the
concentration of sodium chloride increased. This is due to the fact
that as the solute concentration increases, less of the surface area of
the frozen sample is occupied by water. In general, most solutions
or biological samples will have a eutectic temperature of –10° to
–25°C. However, if the sample contains a simple sugar such as
glucose or if the sample is animal or plant tissue, the eutectic
temperature may be as low as –30° to –50°C.
Freeze Dry Capacity

The volume of a sample that can be freeze dried at one time is
related to factors discussed previously and the size and design of
the freeze dry system. With any given instrument, the capacity is
based on the surface area of the sample, the eutectic temperature
and concentration of the sample and the rate and amount of heat
transferred to the frozen sample. Of these factors, the eutectic
temperature is the most important factor in determining the amount
of sample that can be freeze dried at one time, particularly when
flasks are used. This is because as the eutectic temperature
decreases, the vapor pressure decreases but the rate of heat
absorption by the sample does not change. This tends to promote
melting of the sample, which leads to a marked increase in vapor
3
pressure and ultimately overloads the collector and vacuum pump.

Samples that have eutectic temperatures of –20°C or lower should
be placed on the freeze dry system one flask at a time so that the
vacuum in the system may recover before adding another sample
to the system. If the vacuum does not recover, the capacity of the
freeze dry system has been exceeded and the sample should be
removed.
If there is a problem with a particular type of sample melting when

placed on the freeze dry system, dilution of the sample with more
water or providing some insulation around the flask to decrease the
rate of heat absorption by the sample may help. If the eutectic
temperature of the sample is –40 to –60°C, the freeze dry system
selected for use must be equipped with cascade type refrigeration
so that the collector temperature can be cooled to below –75°C, or
a dry ice/solvent trap may be used between the collector and the
vacuum pump.
Samples Containing Volatile

Substances
In certain cases the solvent in a sample to be freeze dried may
contain volatile components such as acetonitrile, methanol, acetic
acid, formic acid or pyridine. In addition to these substances
having an effect on the eutectic temperature, they may increase the
vapor pressure at the surface of the sample. Also, compared to
water, they will require the absorption of less heat for sublimation
to occur. Hence, samples that contain volatile substances will have
a greater tendency to melt, particularly when placed in flasks or
exposed to room temperature. If a sample containing a volatile
substance tends to melt when placed on a freeze dry system,
dilution of the sample with more water will help keep the sample
frozen. For example, a 0.2M solution of acetic acid is much easier
to freeze dry than a 0.5M solution.
About This Manual

This manual is designed to help you learn how to install, use, and
maintain your Freeze Dryer. Instructions for performing routine
maintenance and making minor modifications to your Freeze Dryer
are also included.
Chapter 1: Introduction provides a brief overview of the Freeze

Dryer, explains the organization of the manual, and defines the
typographical conventions used in the manual.
4
Chapter 2: Prerequisites explains what you need to do to prepare

your site before you install your Freeze Dryer. Electrical
requirements are discussed.
Chapter 3: Getting Started contains the information you need to

properly unpack, inspect and install your Freeze Dryer.
Chapter 4: Using Your Freeze Dryer discusses the basic operation

of your Freeze Dryer. Information on how to attach samples and
run the Freeze Dryer is included.
Chapter 5: Maintaining Your Freeze Dryer explains how to

perform routine maintenance on your Freeze Dryer.
Chapter 6: Using the RS232 Receptacle describes how to connect

a computer for monitoring the operation.
Chapter 7: Troubleshooting contains a table of problems you may

encounter while using your Freeze Dryer, including the probable
causes of the problems, and suggested corrective actions.
Chapter 8: Modifying Your Freeze Dryer Display describes how

to calibrate the vacuum display restore factory settings.
Appendix A: Freeze Dryer Components contains labeled diagrams

of the components of the Freeze Dryer.
Appendix B: Freeze Dryer Dimensions contains comprehensive

diagrams showing the dimensions for the Freeze Dryer.
Appendix C: Freeze Dryer Specifications contains product

specifications. A wiring diagram for the Freeze Dryer is also
included.
Appendix D: Freeze Dryer Accessories lists the part numbers and

descriptions of all of the accessories available for your Freeze
Dryer.
5
Typographical Conventions
Recognizing the following typographical conventions will help
you understand and use this manual:
• Book, chapter, and section titles are shown in italic type (e.g.,
Chapter 3: Getting Started).
• Steps required to perform a task are presented in a numbered
format.
• Comments located in the margins provide suggestions,
reminders, and references.
• Critical information is presented in boldface type in paragraphs
! that are preceded by the exclamation icon. Failure to comply
with the information following an exclamation icon may result
in injury to the user or permanent damage to your Freeze
Dryer.
•
☞ Important information is presented in capitalized type in
paragraphs that are preceded by the pointer icon. It is
imperative that the information contained in these paragraphs
be thoroughly read and understood by the user.
6
CHAPTER 2
PREREQUISITES
Before you install your Freeze Dryer, you need to prepare your site
for installation. Carefully examine the location where you intend
to install your Freeze Dryer. You must be certain that the area is
level and of solid construction. An electrical source must be
located near the installation site.
Carefully read this chapter to learn:
• the electrical supply requirements.

• the vacuum pump requirements.
Refer to Appendix C: Freeze Dryer Specifications for complete

Freeze Dryer electrical and environmental conditions,
specifications and requirements.
Electrical Requirements
The Freeze Dryer requires a dedicated electrical outlet. This outlet
requires a 20 Amp circuit breaker or fuse for models rated at 115V
(60 Hz). An outlet equipped with a 15 Amp circuit breaker or fuse
is required for models rated at 230V (50/60 Hz). The power cord
on 115V models is equipped with a 20 Amp NEMA 5-20P plug.
The power cord on 230V models is equipped with a NEMA 6-20P
plug. If this does not match with the available receptacle, remove
this plug and replace it with an approved plug of the suitable style.
7
Chapter 2: Prerequisites
Location Requirements
The Freeze Dryer should be located in an area that provides an
unobstructed flow of air around the cabinet. This air cools the
refrigeration system. The refrigeration system draws air in through
the sides and exhausts it through the rear. A minimum of 3" must
be allowed between the rear and both sides of the Freeze Dryer and
adjacent wall surfaces. Restriction of airflow during operation
could adversely affect performance.
Refer to Appendix C: Freeze Dryer Specifications for dimensional

drawings of the Freeze Dryer.
Vacuum Pump Requirements

A vacuum pump must be provided by the user. A vacuum pump
with a displacement of 144 liters per minute and 0.0002 mBar
ultimate pressure is adequate for most samples. The inlet fitting on
the vacuum pump must be suitable for 3/4" ID vacuum hose,
which is provided. It is recommended that the vacuum pump is
equipped with an exhaust filter to minimize oil mist exhausting
from the vacuum pump. The operating vacuum level may be set
on the Freeze Dryer. The higher the pressure is set, the more likely
it is that oil mist will be exhausted.
Vacuum pumps used with 115V models should be equipped with

an 115V, 15 Amp NEMA 5-15P plug. Vacuum pumps used with
230V models should be equipped with a reverse IEC plug. This
plug is included with 230V models. This will allow the vacuum
pump to be plugged into the receptacle on the back panel of the
freeze dryer. See Appendix D: Freeze Dryer Accessories for
vacuum pumps available from Labconco.
Chamber or Manifold
Requirements
A freeze drying chamber is not included and must be purchased
separately. These allow samples to be attached to the Freeze
Dryer. See Appendix D: Freeze Dryer Accessories for available
chambers and manifolds.
8
CHAPTER 3
GETTING STARTED
Now that the site for your Freeze Dryer is properly prepared, you
are ready to unpack, inspect, install and test your Freeze Dryer.
Read this chapter to learn how to:
• unpack and move your Freeze Dryer.

• set up your Freeze Dryer.
• connect the electrical supply source to your Freeze Dryer.
• properly exhaust your Freeze Dryer.
• safely use solvents with your Freeze Dryer.
The FreeZone Freeze Dry System may weigh as

! much as 330 lbs. (150 kg) depending upon the
model. If you must lift the Freeze Dryer
manually, use at least two (2) persons and follow
safe lifting guidelines.
Unpacking Your Freeze Dryer

Carefully unpack your Freeze Dryer and inspect it for damage that The United States
may have occurred in transit. If your Freeze Dryer is damaged, Interstate Commerce
notify the delivery carrier immediately and retain the entire Commission rules
require that claims be
shipment intact for inspection by the carrier. filed with the delivery
carrier within fifteen (15)
DO NOT RETURN GOODS WITHOUT THE
☞
days of delivery.
PRIOR AUTHORIZATION OF LABCONCO.
UNAUTHORIZED RETURNS WILL NOT BE
ACCEPTED.
9
Chapter 3: Getting Started
IF YOUR FREEZE DRYER WAS DAMAGED IN

☞ TRANSIT, YOU MUST FILE A CLAIM
DIRECTLY WITH THE FREIGHT CARRIER.
LABCONCO CORPORATION AND ITS
DEALERS ARE NOT RESPONSIBLE FOR
SHIPPING DAMAGE.
☞
DO NOT DISCARD THE CARTON OR
PACKING MATERIAL FOR YOUR FREEZE
DRYER UNTIL YOU HAVE CHECKED ALL OF
THE COMPONENTS AND INSTALLED AND
TESTED THE FREEZE DRYER.
Freeze Dryer Components

Locate the model of Freeze Dryer you received in the following
table. Verify that the components listed are present and
undamaged.
Catalog Numbers 6, 12 and 18 Liter Console Models

Teflon
Catalog Coated Purge Drying Shell
Number Description Volts Hz Chamber Valve Chamber Freezer
7753020 6 Liter Freeze Dryer 115 60

7753021 6 Liter Freeze Dryer 115 60 x
7753024 6 Liter Freeze Dryer 115 60 x x
7753027 6 Liter Freeze Dryer 115 60 x x x

10

Teflon
7934020 6 Liter Cascade Freeze Dryer 115 60
7934021 6 Liter Cascade Freeze Dryer 115 60 x
7934024 6 Liter Cascade Freeze Dryer 115 60 x x
7934027 6 Liter Cascade Freeze Dryer 115 60 x x x


11

Teflon
Plus the Following:

Part # Component Description
7403400 User’s Manual
1336400 Power Cord – 115V
or
1342100 Power Cord – 230V
1291000 Plug (230V models only)
7646000 Vacuum Hose
1967600 Hose Clamps (2)
7532900 Collector Chamber Lid
7690800 Collector Chamber Lid Gasket
7408300 Drying Chamber Lid (if so equipped)
7408400 Drying Chamber and Shell Freezer Lid Gasket (if so equipped)
7403100 Shell Freezer Lid (if so equipped)
1429900 Stopper (with Drying Chamber only)
7390702 Baffle (6L Cascade only)
7390701 Baffle (12L Cascade only)
7390700 Baffle (18L Only)
If you did not receive one or more of the components listed for
your Freeze Dryer, or if any of the components are damaged,
contact Labconco Corporation immediately for further instructions.
Setting Up Your Freeze Dryer

After you verify receipt of the proper components, move your
Freeze Dryer to the location where you want to install it. Then,
follow the steps listed below.
12
Vacuum Pump Connection

A vacuum pump as described in Chapter 2: Prerequisites is
required to operate your Freeze Dry System properly. The Freeze
Dryer is equipped with a 3/4" ID, heavy wall, vacuum hose for
connecting the collector chamber to the vacuum pump.
Make certain that the oil in the vacuum pump is

! at the proper level.
Remove the front stainless steel panel or lower rear panel from the
Freeze Dryer. The front panel is removed by placing a flat blade
screw driver into the rectangular hole in the center of the kick
panel. Pivot the handle downward to disengage the latch and
simultaneously pull the lower panel forward.
Place the vacuum pump inside the cabinet. Connect the vacuum
pump power cord to the receptacle on the back of the cabinet
labeled “vacuum pump.” Models rated for use on 230V have a
reverse IEC connector for attaching the vacuum pump power cord.
A plug is supplied that can be installed on the vacuum pump power
cord if necessary. If the vacuum pump has an off/on switch, turn
the switch on. The vacuum pump will be controlled by the Freeze
Dryer. Connect the vacuum pump inlet port to the vacuum tube
inside the cabinet near the front with the vacuum hose and clamps
provided. If necessary, cut the hose to proper length to allow for
gentle bends without kinks.
Optional Purge Valve
Vacuum Hose
13
The lower front panel is installed by first sliding the top edge under
the lip on the plastic control panel. Pivot the bottom inward and
push until the latch is secure.
Electrical Connection
Plug the power cord into the receptacle on the back of the Freeze
Dryer and plug the other end into a suitable power receptacle.
Drying Chamber or Drying Manifold

Installation
The drying chamber or drying manifold, purchased separately, may
be positioned directly above the 3-inch port on the top of the
Freeze Dryer. Follow the instructions supplied with the selected
accessory.
Chemical Resistance of Freeze Dryer

Components
The FreeZone Freeze Dry System is designed to be chemically
resistant to most compounds that are commonly used in freeze
drying processes. However, by necessity, the Freeze Dryer is
comprised of a number of different materials, some of which may
be attacked and degraded by certain chemicals. The degree of
degradation is dependent on the concentration and exposure
duration. Some of the major components of the FreeZone Freeze
Dry System that are susceptible to degradation are as follows:
14
Acids Buffers Solvents
Methyl t-Butyl Ether (BTBE)

Trifluoroacetic Acid (TFA)
Carbon Tetrochloride
Sodium Phosphate
Calcium Chloride
Acetic Acid 20%
Cyclohexane
Acetonittirle
Formic Acid
Pyridine
Dioxane
Acetone
Component Material
Valve Stem Acetal C D D D D
(Delrin)
Collector* Acrylic D D D D
Lid
Hoses, Neoprene C D D C C D D D C D
Gaskets &
Valve
Bodies
Flask Top Silicon C D D D D D C D
Rubber
Chamber & Stainless C
Fittings Steel
* An accessory glass lid is available.

C – Moderate degradation; Limited use.
D – Severe degradation; infrequent use recommended; immediate
thorough cleaning required.
• Most common compounds used in freeze drying processes, if

allowed to enter the vacuum pump, will degrade the oil and
cause damage to the vacuum pump.
• Sugars and proteins typically will have minimal negative effect

on any of the materials of construction.
When using compounds in the Freeze Dryer that are hostile to the
materials of construction, it is imperative the equipment is
thoroughly cleaned after use.
15
• Rubber and plastic components that have been exposed to

damaging compounds should be removed and flushed with
water.
• The oil in the vacuum pump should be checked often. It must
be changed if it is cloudy, shows particles or is discolored. The
useful life of vacuum pump oil can be extended if the vacuum
pump is operated for an extended period of time after a freeze
dry run. This allows contaminants to be purged from the hot
oil. This must be done with the inlet to the pump blocked off
to prevent air from free flowing through the pump. This is
accomplished by closing all sample valves on a clean, dry
freeze dry system and turning on the vacuum pump. If the
pump is operated at an elevated vacuum level (> 10mBar), oil
may be expelled from the pump and damage could occur.
Another way to extend the life of the vacuum pump is to install an

optional secondary trap in the line between the Freeze Dryer and
the vacuum pump. Contact Labconco for ordering information.
With prudent maintenance the FreeZone Freeze Dry System will

provide years of service. Warranty on the affected parts will be
voided if maintenance has been obviously neglected. If you have
questions about using specific compounds in the Freeze Dryer,
contact Labconco Technical Service at 1-800-821-5525 or 816-
333-8811 or e-mail: labconco@labconco.com.
Solvent Safety
! Precautions
Solvents used in the Freeze Dryer may be
flammable or hazardous to your health. Use
extreme caution and keep sources of ignition
away from the solvents. When using flammable
or hazardous solvents, the vacuum pump must
be vented to a fume hood.
Hazardous materials such as strong acids or

bases, radioactive substances and volatile
organics must be handled carefully and
promptly cleaned up if spilled. If a sample is
spilled in the collector chamber it must
immediately be cleaned up.
16
WARNING: The disposal of substances used in

connection with this equipment may be governed
by various Federal, State or local regulations.
All users of this equipment are urged to become
familiar with any regulations that apply in the
user’s area concerning the dumping of waste
materials in or upon water, land or air and to
comply with such regulations.
17
CHAPTER 4
USING YOUR FREEZE
DRYER
After your Freeze Dryer has been installed as detailed in Chapter 3:
Getting Started, you are ready to begin using your Freeze Dryer. Read
this chapter to learn how to:
• operate the controls.

• understand the display.
• connect samples.
Do not use the Freeze Dryer in a manner not specified
! by the manufacturer (refer to Appendix C: Freeze Dryer

Specifications). The electrical protection properties of
the Freeze Dryer may be impaired if the Freeze Dryer is
used inappropriately.
18
Chapter 4: Using Your Freeze Dryer
Freeze Dryer Controls

The control panel for the Freeze Dryer is shown below with a description
about its function.
1 15 19 2 10
5 17
11
9
8
12
3
18
6 4 14 16
1. LCD Display – Displays system operating parameters, set-up

parameters and alarm messages.
2. Menu Switch – This switch is used to change the display from
operating system parameters to set-up parameters.
3. Select Switch – Used to select set-up parameters.
4. Vacuum Switch – Used to start or stop the vacuum pump when operating in
manual start-up mode.
5. Vacuum Indicator – This green LED indicates that power is being supplied to
the vacuum pump receptacle on the back of the Freeze Dryer.
6. Manual Refrigeration Switch – Used to start only the refrigeration module.
7. Manual Operation Indicator – When lit, the green LED indicates the Freeze
Dryer is being controlled manually by the operator. The operator must start
each function.
8. Auto Mode Switch – Used to start or stop the refrigeration and the Auto Mode
process.
19
9. Auto Mode Indicator – When lit, the green LED indicates that the Freeze Dryer
is in Auto Mode. In this mode, the vacuum pump will start when the collector
temperature reaches –40°C.
10. Vacuum Graph Display – This display indicates the relative system vacuum
level. The highest LED indicates that the vacuum level is above 2.0 mBar.
The indicators will sequence down when the vacuum level reaches 2.0, 1.0,
0.8, 0.6, 0.45, 0.12 mBar. The lower green LED flashes when the system
vacuum level is 0.45 to 0.12 mBar and illuminates steadily below 0.133 mBar.
11. Collector Temperature Graph Display – This display indicates the temperature
of the collector. The highest LED indicates the collector temperature is
warmer than 10°C. The indicators will sequence down when the temperature
reaches 10, 0, -10, -20, -30, -40°C. When the collector temperature is –40°C or
lower the green indicator will light.
12. Alarm Indicator – This red LED indicates that a system alarm has occurred.
Press the Menu Switch to display the alarm message on the LCD display.
13. Main Power Switch – Turns the Freeze Dryer on or off. (Not shown, located
on the left side of the cabinet.)
14. Defrost Switch – Used to defrost ice from the collector coil.
15. Defrost Indicator – This green LED illuminates when the Freeze Dryer is in
defrost mode.
16. Purge Valve Switch – Used to open or close the purge valve, if the model is so
equipped.
17. Purge Valve Indicator – This green LED illuminates when the purge valve is
closed.
18. Shell Freezer/Vacuum Chamber Switch – Used to operate the shell freezer or
the heater on the vacuum chamber if the model is so equipped.
19. Shell Freezer/Vacuum Chamber/Indicator – This green LED illuminates when

either the shell freezer or vacuum chamber heater is operating.
20
Operation Checklist
The following checklist should be followed prior to each use of your
Freeze Dryer:
1. Wipe the interior of the collector chamber with a soft cloth or paper
towel to remove any accumulated moisture.
2. Check the collector chamber drain hose to ensure that the hose is free
of moisture and that the drain plug is securely installed. The Freeze
Dryer will not start if moisture is detected.
3. Using a soft, lint-free cloth or paper towel, wipe the collector chamber
lid gasket to remove any dirt and contaminants that could cause a
vacuum leak. Vacuum grease is not required on the lid gasket to
obtain a proper vacuum seal.
4. Remove the accessory drying chamber or manifold from the
connection port and using a soft, lint-free cloth or paper towel, wipe
the port gasket and sealing surfaces of the drying chamber/manifold to
remove any dirt and contaminants that could cause a vacuum leak.
Reinstall the drying chamber or manifold on the port. Vacuum grease
is not required on the port gasket to obtain a proper vacuum seal.
5. Inspect each sample valve on the accessory drying chamber or
manifold and check for any visible damage and for improper
installation that might cause a vacuum leak. Also check that each
sample valve is closed or in the “vent” position.
Vacuum Pump Ballast Setting

Most vacuum pumps are equipped with a gas ballast mechanism. The
freeze dry process requires high vacuum. Therefore, it is recommended
that the gas ballast be closed during the operation of the Freeze Dry
System. If the gas ballast is left open for extended periods of operation,
the oil can be pumped out the exhaust, causing the pump to fail.
Purge Valve
The optional purge valve is installed between the Freeze Dryer collection
chamber and the vacuum pump. When the green LED above the PURGE
switch is illuminated, the purge valve is closed and the vacuum pump is
isolated from the Freeze Dryer collection chamber.
During Freeze Dryer start-up, the refrigeration system pulls the collector
coil down to temperature. While the collector coil cools, the purge valve
can be closed and the vacuum pump allowed to
run. This allows the vacuum pump oil to warm, which will evaporate and
expel condensed solvents from the oil. When the collector coil is down to
21
temperature and the freeze dry process is started, the warm pump oil is
less likely to condense solvent vapors that are not trapped by the collector
coil. When the Freeze Dryer is operated in the Automatic Mode, the
purge valve and vacuum pump will operate automatically to perform this
function. In the Manual Mode the user must manually activate the purge
valve and vacuum pump to perform this function.
During shut down the vacuum pump can be run for several minutes with
the purge valve closed. This will allow the warm pump oil to evaporate
and expel solvent vapors that condensed in the pump oil during the freeze
dry process. Whether the Freeze Dryer is run in the Automatic Mode or
the Manual Mode, the user must manually activate the purge valve and
vacuum pump to perform this function.
If power to the Freeze Dryer is interrupted during the freeze dry process,
the purge valve will open during the power outage, and the vacuum bleed
valve will open to allow atmospheric air to enter the system.
Operating the Freeze Dryer

Set-Up
The Freeze Dryer may be configured to automatically start the vacuum
pump when the collector temperature reaches –40°C. The display units
for vacuum may be selected to be mBar, Pascal (Pa) or Torr and the
temperature may be displayed as °F or °C. The run time of the
refrigeration system and the vacuum pump may be monitored.
To configure your Freeze Dryer, turn the main power switch ON and press
MENU. The display will show:
VACUUM UNITS
mBar Pa Torr
• Press SELECT until the desired units are flashing.

• Press MENU.
• The display will show:
VACUUM SET POINT
XXXX YYY
Where YYY is the units selected above.
22
• Press SELECT until the desired vacuum operating level is

displayed. See “Setting the Operating Vacuum Level” for
guidelines.
• If “0” is selected, the vacuum control is disabled and the vacuum
level in the Freeze Dry System will be determined by the
capabilities of the vacuum pump.
• Press MENU.
TEMPERATURE UNITS
°C °F
Press SELECT until the desired units are flashing is displayed.

Press MENU.
The display will show the following screen if the Freeze Dryer is equipped
with a Drying Chamber.
DRYING CHAMBER SETPOINT:
XX Y
When Y is the units selected above.

• Press SELECT until the desired temperature is displayed.
• Press MENU.
REFRIG TOTAL HOUR: XXXX

SERVICE HOUR: XXXX
• To reset the SERVICE HOUR to 0 press SELECT. This allows

you to keep track of the time the refrigeration system operated
since it was serviced.
• The display will show the refrigeration system hours.
REFRIG TOTAL HOUR: XXXX

RESET SERVICE HOUR: ?
23
• To reset the service hours to 0, continue to hold SELECT 5

seconds until hours are reset.
• TOTAL HOUR cannot be reset.
• Press SELECT.
• The display will show the vacuum pump hours.

VACUUM TOTAL HOUR: XXXX
SERVICE HOUR: XXXX
• To reset the SERVICE HOUR to 0, press SELECT.

VACUUM TOTAL HOUR: XXXX
RESET SERVICE HOUR: ?
If you want to reset the service hours to 0, continue to hold SELECT five
seconds until hours are reset.
• Press SELECT.
• The display will show the RS-232 data transmission rate.
RS-232 TRANSMISSION RATE
10 SECONDS
• To change the rate press and hold SELECT until the desired time
interval is shown. The time between data transmissions may be set
to occur at 10, 30, 60, 300 or 600 second intervals.
• Press SELECT to return to display operating parameters or after a
short delay, the display will automatically switch to show
operating parameters.
24
Baffle
(6 Liter –84°C Cascade model, 12 Liter –84° Cascade model & 18
Liter Model)
Position the baffle so it rests on the top of the collector coil. The arrow
should point toward the front.
Automatic Start-Up
(Models not equipped with a purge valve)
To run the Auto Mode, press the panel switch labeled REFRIGERATION
AUTO. The green LED above the switch will illuminate. This will start
the refrigeration system. When the collector reaches –40°C, the vacuum
pump will start. The Temperature and Vacuum Graphs will indicate
collector temperature and system vacuum. The LCD display will show the
actual temperature of the collector. When the vacuum in the system is
above 5 mBar the vacuum display will indicate “HI.” At 5 mBar and
below, the display will show the actual vacuum.
When the system vacuum is between 0.450 and 0.133 mBar, the lower
green vacuum graph LED will flash. When the system vacuum level is
<0.133 mBar, the green LED will be lit steadily indicating that most
samples may be added.
Automatic Start-Up
(Models equipped with a purge valve)
To run the Auto Mode, press the panel switch labeled REFRIGERATION
AUTO. The green LED above the switch will illuminate. The LED’s
above the vacuum and purge switches will also illuminate. The
refrigeration system and vacuum pump will start and the purge valve will
close. When the collector reaches
–40°C, the purge valve will open. The Temperature and Vacuum Graphs
will indicate collector temperature and system vacuum.
The LCD display will show the actual temperature of the collector. When
the vacuum in the system is above 5 mBar the vacuum display will
indicate “HI”. At 5 mBar and below, the display will show the actual
vacuum. When the system vacuum is between 0.450 and 0.133 mBar, the
lower green vacuum graph LED will flash. When the system vacuum
level is <0.133 mBar, the green LED will be lit steadily indicating that
most samples may be added.
25
Manual Start-Up
(Models not equipped with a purge valve)
To manually run the freeze dry process, press the REFRIGERATION
MAN switch. This will start the refrigeration system. The green LED
above the switch will illuminate. When the collector temperature reaches
–40°C, the vacuum pump may be started by pressing the VACUUM
switch. The Temperature and Vacuum Graphs will indicate collector
temperature and system vacuum. The LCD display will show the actual
temperature of the collector. When the vacuum in the system is above 5
mBar the vacuum display will indicate “HI.” At 5 mBar and below, the
display will show the actual vacuum.
<0.133 mBar, the green LED will be lit steadily indicating that samples
may be added.
Manual Start-Up
(Models equipped with a purge valve)
To manually run the Freeze Dryer, press the REFRIGERATION MAN

switch. The green LED above the switch will illuminate. The PURGE
switch and VACUUM switch may be pressed. LED’s above the switches
will illuminate. The purge valve will close and the vacuum pump will
start. (Do not start the vacuum pump without first closing the purge
valve). When the collector temperature reaches –40°C or any time
afterwards, press the PURGE switch to open the purge valve. The
Temperature and Vacuum Graphs will indicate collector temperature and
system vacuum. The LCD display will show the actual temperature of the
collector. When the vacuum in the system is above 5 mBar the vacuum
display will indicate “HI”. At 5 mBar and below, the display will show
the actual vacuum.
<0.133 mBar, the green LED will be lit steadily indicating that samples
may be added.
26
Setting the Operating Vacuum Level

The vacuum level may be set by the user to optimize the freeze dry
process. Normally, the sublimation rate will increase if there is less
vacuum (a higher pressure) in the Freeze Dryer. A good starting place is
to set the vacuum so its level is equivalent to about 10°C colder than the
eutectic or collapse temperature of the sample. Adjustments to the
vacuum level must be made for various freeze drying conditions. Factors
that must be considered are whether the sample is freeze dried on heated
shelves or in glassware attached to manifold valves, the volatility of the
sample itself, the size of the sample and the heat energy supplied to the
sample.
When the vacuum control is set to operate at less vacuum, the ice holding
capacity of the collector may be decreased. This can be improved in non-
cascade models by installing a baffle in the collector. See Appendix D
Freeze Dryer Accessories for the baffle part number. See the section titled
Baffle in this chapter for proper installation.
Some guidelines for setting the Freeze Dryer are shown below. These
show pre-freezing temperatures and vacuum levels. Exact protocols must
be determined by the user for the specific samples that are being freeze
dried.
Solidification/Eutectic Pre-Freeze
Material Vacuum Set Point
Temperature Temperatures
Bacteria,Virus -40°C and Colder -50°C & 0.040 mBar &
Colder Lower
Milk -5 to -13 -15 to -23 1.65 to 0.77
Fungi -40 and Colder -50 & Colder 0.04 and lower
Vegetable Tissue -25 to -50 -35 to -60 0.22 to 0.01
Human Tissue -30 to –40 -40 to –50 0.12 to 0.04
Blood Plasma -10 to –25 -20 to –35 1.03 to 0.22
Vaccine -30 to –40 -40 to –50 0.12 to 0.04
Pre-Freezing Samples
Appropriate containers for freeze drying include ampules, serum bottles,
and wide mouth freeze drying flasks. Shell freezing of samples is
recommended for wide mouth freeze drying flasks. Smaller samples in
ampules and serum bottles may be frozen in a freezer. The sample
container size should always be at least two to three times the sample size
(i.e., 40 ml samples should be prepared in 80 ml containers or larger). The
temperature required for pre-freezing is dependent on the characteristics of
the sample. Pre-freezing temperature typically is at least 10° to 20°C
below the eutectic or collapse temperature of the sample.
27
Adding Sample
The following procedure should be followed when using sample valves in
the freeze dry process:
1. Connect a pre-frozen sample to a sample valve on the drying chamber or

manifold using an adapter. Turn the plastic valve knob to the “VACUUM”
position to open the valve. The bevel on the knob should be positioned
toward the sample port to apply vacuum to the sample.
Bevel in “vent” position
Vent/Backfill Port
Bevel in “vacuum”
position
Adapter
2. Before adding another sample, allow system vacuum to return to 0.133

mBar or lower. Any combination of valves and sample sizes may be
utilized at one time provided that the system vacuum and collector
temperature remain sufficiently low to prevent melting of the frozen
sample.
3. When all the frost has disappeared from the outer surface of the
sample container and no cold spots can be detected by handling the
container, the sample is nearly dry. To be certain of low final moisture
content, dry the sample for several hours past this point.
4. To remove a container after drying is complete, turn the plastic knob
on the valve to the “VENT” position, which closes the valve and vents
the container. Should backfilling with an inert gas be required,
connect the gas supply line to the vent port on the valve before turning
the plastic knob on the valve to vent
28
position. The sample container may now be removed. In the vent

position the bevel on the valve knob should point away from the
sample port.
5. Ampules may be flame sealed while connected to a valve by using a
sealing torch. Care must be taken not to burn the valve. An insulation
material placed between the valve and the torch is recommended.
Shut Down
At the end of a run or when a sufficient amount of condensate accumulates
on the collector coil to obstruct the flow of vapor to the collector chamber,
the Freeze Dryer should be defrosted. First, release system vacuum by
turning the plastic knob on a valve to the open position or by pulling the
collector chamber drain plug out of the drain hose. Now press the
Vacuum Switch on the control panel to turn the vacuum pump OFF. Press
the Refrigeration Switch next to the illuminated LED to turn OFF the
refrigeration system. Turn OFF the Main Power Switch on the left hand
side of the cabinet.
After a run is complete, it may be desirable to purge contaminants from

the vacuum pump oil. This can be accomplished by first closing the purge
valve by pressing the purge switch. The LED will illuminate. Then turn
on the vacuum pump by pressing the vacuum switch, let the pump operate
for an extended period of time.
Defrosting
The following procedure should be followed when defrosting the collector
coil:
1. Pull the collector chamber drain hose out from the front panel of the
unit and remove the drain plug. Place the drain hose in a suitable
container to collect the condensate that will be defrosted off the
collector coil.
2. Press the DEFROST switch on the control panel. The green LED
above that switch will illuminate. Allow unit to operate in this
condition until all condensate is defrosted from the collector coil.
Dispose of the liquid appropriately.
3. Lift out the ice plug after it has melted sufficiently to be removed
without force.
4. Flush the collector chamber with water and wipe chamber dry.
5. If rapid defrost is desired, pour warm water into the collector chamber
covering no more than the bottom 2 coils. If excess
water is added it can enter the vacuum port and drain into the
vacuum pump.
29
6. Press the DEFROST switch, the green LED will be off. Reinstall the
drain hose plug and slide drain hose back into cabinet through the front
panel. Dispose of the liquid appropriately.
Utilization of acid requires immediate cleaning and

! neutralization after defrost or physical damage to the
collector chamber and collector coil will result.
Do not attempt to chip ice from the collector coil as

damage may occur to the coil.
Never attempt to start the vacuum pump when there is

liquid in the collector chamber. This could result in
damage to the vacuum pump.
Operating the Shell Freezer

The optional built in shell freezer is designed for shell freezing samples in
flasks in preparation for freeze drying.
Follow the steps below each time you use the shell freezer to obtain
optimum performance:
1. Check that the solvent bath drain plug is securely installed in the drain
hose.
2. Remove the bath compartment cover and add solvent to the bath
compartment. Commonly used solvents are methanol or ethanol.
Recommended solvent depth is ¼" to ½" above the top of the rollers
(approximately 2 liters).
If flammable solvents are used in the shell freezer bath,

! be sure to keep away from open flame.
3. Press the panel switch labeled SHELL FREEZE. The green LED
above the switch will illuminate. The shell freezer refrigeration
module will start and the bath rollers will begin rotating. The LCD
display will show the shell freezer bath temperature.
4. Fill a freeze dry container no more than ½ full with sample and stopper
the container top. Lay the container on the rollers in a
horizontal position. Replace the bath compartment cover during shell

freezing.
5. When the sample is completely frozen in the container, remove the
container from the bath compartment and freeze dry the sample or
place it in a suitable storage freezer for future freeze drying.
6. Press the SHELL FREEZE switch to turn shell freezer off.
30
7. If the Shell Freezer is to be used for cold bath operation, additional

solvent may be added to submerge small flasks. Do not fill pan more
than 2 inches below the top of the stainless steel pan with vessels
submerged. Allow additional time for larger volumes of solvent to
pull down in temperature.
8. Always drain flammable solvents from the bath when the shell freezer
is not in use and store the solvent in a suitable container. This is
accomplished by first pulling the drain hose out of the front panel of
!
the unit and then removing the drain plug. Place the hose in a suitable
container to collect the solvent.
Operating the Vacuum Drying

Chamber
The built-in drying chamber is designed for freeze drying small samples,
either in bulk or in small containers such as vials or 96 well plates. It may
be used in conjunction with other drying accessories that are mounted on
top of the Freeze Dryer or independently. If a manifold or chamber is
mounted to the Freeze Dryer and is not in use, close all of its valves. If no
drying accessory is installed on the Freeze Dryer, place the supplied
stopper in the center of the 3.0 accessory port that is on the top of the
Freeze Dryer to seal the vacuum system. Follow the steps below to
operate the built-in drying chamber.
1. Start the Freeze Dryer. Position the Vacuum Chamber valve on the
top of the Freeze Dryer to the VENT position. Turn on the
refrigeration in the Freeze Dryer in the MAN or AUTO mode
according to the instructions in this manual. If the sample will be
prefrozen in the collector chamber, the Freeze Dryer must be started in
the MAN mode.
2. Set the Drying Chamber temperature according to the Set Up
instructions in this manual. The set temperature should be lower than
the eutectic temperature of the sample.
NOTE: The Drying Chamber is NOT refrigerated. If the operating
temperature is set below ambient, the only source cooling the chamber
is the sample itself.
31
3. Press the switch marked Shell Freezer/Vacuum Chamber to actuate the

heater.
4. Freeze the sample. Before the freeze dry process can occur, the
product to be freeze dried must be in a frozen state. This can be done
in a separate freezer or in the Freeze Dryer collector chamber.
5. Load the samples. The Freeze Dryer collector temperature must be –
40°C or colder. Replace the chamber lid.
6. Start primary drying. Turn the vacuum control valve on the top of the
Freeze Dryer to VACUUM. Start the vacuum pump if the Freeze
Dryer was started in the MAN mode.
7. Start secondary drying. After all the free moisture is removed in the
primary drying phase, the temperature of the chamber may be
increased. Do this according to the instructions in the Set Up section
of this manual.
8. Shut Down. After completion of the freeze dry procedure:
a. Press the Shell Freezer / Vacuum Chamber Switch to turn off
the chamber heater.
b. Release vacuum in the chamber by turning the valve on the top
of the Freeze Dryer to VENT.
c. Remove the sample.
d. Release vacuum from the Freeze Dryer by either opening the
Vacuum Chamber valve when the chamber lid is off or by
removing the drain plug or by opening a valve on chamber or
manifold mounted on top of the Freeze Dryer. Turn off the
vacuum pump.
e. Turn off the Freeze Dryer, defrost and drain the chamber per
instructions in this manual.
Alarms
A number of unusual events may occur during a lyophilization procedure
that can adversely effect the operation of the Freeze Dryer. If an event
occurs, the alarm indicator will flash and the beeper will sound.
The beeper will automatically mute itself after one minute. The specific
alarm can be identified by pressing MENU. Pressing MENU multiple
times will display multiple alarms if they have occurred. The following
“out of specification” conditions will initiate an alarm:
Power Failure
If a power failure occurs during a Freeze Dry process, the vacuum control
valve will allow air to bleed into the Freeze Dryer System.
32
If the failure is of a short duration and the collector does not warm up
excessively, when power is restored, the Freeze Dryer will restart and
resume operation of the refrigeration and vacuum systems. If the power
failure lasts for a longer duration and the collector warms above safe
limits, when the power is restored, the Freeze Dryer will not restart by
itself. This prevents melted sample from being drawn into the collector
and prevents liquid from being sucked into the vacuum pump. When
power is restored, the alarm indicator will flash and the alarm beeper will
sound. When the MENU button is pressed the display will show
POWER FAIL
HOLD SELECT TO CLEAR IT
Press and hold SELECT for five seconds until the error message is cleared
from the display.
Line Voltage Out of Range

If the voltage supplied to the Freeze Dryer varies beyond allowable limits,
the alarm will be activated. When an alarm occurs, press MENU and the
display will show:
LINE VOLTAGE ERROR
The alarm will self-cancel when the proper voltage is restored. The high
and low alarm points are preset at the factory to correspond to the normal
allowable voltage variations based on the nominal voltage specified for the
freeze dryer. Some models may be operated outside the normal voltage
limits. See Appendix C.
If necessary, the high and low alarm points may be adjusted for these
models. See Chapter 8.
Temperature Out of Range

An alarm will be activated if the collector temperature rises above –40°C.
If this occurs, the display will show:
COLLECTOR TEMPERATURE
from the display.
33
Service Vacuum Pump

The vacuum pump normally plugs into the vacuum pump electrical
receptacle on the back of the Freeze Dryer. When the Freeze Dryer has
accumulated a total of 1000 operating hours, the alarm indicator will flash.
Press MENU to display the alarm:
CHANGE VACUUM OIL

from the display.
This will reset the 1000 hour timer. It may be necessary to service the
vacuum pump more frequently than every 1000 hours depending on the
operation of the Freeze Dryer. The pump oil should be regularly
monitored to verify that it is clean.
Moisture in Collector
If there is liquid in the collector chamber and either a REFRIGERATION
button or the VACUUM button is pressed, neither function will start and
an alarm will be activated. When MENU is pressed, the display will
show:
MOISTURE IN COLLECTOR
When the collector is drained, the alarm will self-cancel.
This feature prevents the inadvertent start of the vacuum pump when
liquid is in the collector and thereby can extend the life of the vacuum
pump. A few drops of liquid may remain in the drain hose after draining.
When the vacuum pump is started these drops may be sucked into the
collector chamber. This is normal.
34
CHAPTER 5
MAINTAINING YOUR
FREEZE DRYER
Under normal operation, the Freeze Dryer requires little
maintenance. The following maintenance schedule is
recommended:
As needed:
1. Clean up all spills; remove liquids from the chamber.

2. Clean lid and gasket using soft cloth, sponge or chamois and a
mild, non-abrasive soap or detergent.
3. Check oil level of the vacuum pump. It should be between
MIN and MAX. If the oil level is less than an inch (25.4 mm)
above MIN, add oil to proper level.
4. If oil shows cloudiness, particles or discoloration, drain the
pump and replace with fresh oil.
5. Utilization of acids requires immediate cleaning and
neutralization after a run or physical damage to the
collector chamber and collector coil will result.
6. Check the collection chamber for condensed or frozen solvents
and dispose of appropriately. Completely empty the collector
chamber before the next run or before attempting to start the
vacuum pump.
7. If sample valves leak or stems become difficult to turn, pull the
stem out of the rubber valve body and apply a thin coat of
vacuum grease to the stem. Reinsert the stem into the valve
body.
35
Chapter 5: Maintaining Your Freeze Dryer
Monthly:
1. The rubber components on the Freeze Dryer may eventually

deteriorate and require replacement. The effective life of
rubber parts depends upon both their usage and the surrounding
environment. Check all rubber hoses and gaskets and replace
any that show signs of hardening, permanent set or
deterioration.
2. Using a soft cloth, sponge or chamois and a mild, non-abrasive
soap or detergent, clean the acrylic chamber lid.
3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive
soap or detergent, clean the exterior surfaces of the Freeze
Dryer. Liquid spray cleaners and polishes may be used on the
exterior surfaces. Do not use solvents to remove stains from
the exterior surfaces as they may damage the finish.
Annually:
1. Every 12 months, or more often if the Freeze Dryer is operated

in a dusty environment, the refrigeration system condenser
should be cleaned. Using a vacuum cleaner with brush
attachment, clean the condenser to ensure proper airflow for
peak performance.
36
CHAPTER 6
USING THE RS232
RECEPTACLE
The operation of the Freeze Dryer can be monitored using a
computer when it is connected to the RS232 receptacle on the rear
panel. The computer cannot control the operation of the Freeze
Dryer. The monitored parameters are the collector temperature in
°C and vacuum in microbars.
When a Labconco Stoppering Tray Dryer is connected to a

Labconco Freeze Dryer as detailed in the Stoppering Tray Dryer
User’s Manual, the status of the Stoppering Tray Dryer may be
monitored simultaneously with the status of the Freeze Dryer.
Computer Connection for

Computer Interface
Check your computer to see which type of serial port is provided,
then use a connecting cable below:
1. Computers with a 25 pin D-sub male serial connector

should use Connect Cable, Labconco part number 7537801,
to connect a computer to the Labconco Freeze Dryer.
2. Computers with a 9 pin D-sub male serial connector should
use Connect Cable, Labconco part number 7537800, to
connect a computer to the Labconco Freeze Dryer.
The purpose of the RS232 interface is to send data to a data

logging computer to monitor the state and activity of the Freeze
Dryer. This data is half duplex data. The data properties are as
follows:
37
Chapter 6: Using the RS232 Receptacle
1. Data Rate 2400 Baud

2. 8 Bit word length
3. 1 Start bit, 1 Stop bit
4. No parity is transmitted
5. Standard ASCII character set
The time between data transmissions may be varied by the user to

occur at 10, 30, 60, 300 or 600 second intervals. Press the MENU
button until the RS232 screen appears on the display.
RS-232 TRANSMISSION RATE
10 SECONDS
Press select until the desired time interval is shown.
The format of the transmitted message is as follows:
B<T= -48 V= 18 SF = 999 C=999 PG=9 >
Where:
B = Base Unit
T = Collector Temperature
-48 = Collector Temperature in °Celsius
V = Vacuum
18 = Vacuum Level in Micro Bars
SF = Shell Freezer Temperature (if so
equipped)
9 = Feature not installed or out of range
C = Vacuum Chamber Temperature (if so
equipped)
PG = Purge (if so equipped)
1 = On
0 = Off
If a Stoppering Tray Dryer is attached to the Freeze Dryer and the

data interconnect cable is installed, additional data about that
accessory will be transmitted from the Freeze Dryer. See the
User’s Manual for the Stoppering Tray Dryer for a description of
the data.
There are several commercially available software packages,

which can read RS232 data and enter the data into a computer
program such as a word processor (to create a text file) or
38
spreadsheet (to tabulate and plot the data). Consult your laboratory
supply dealer regarding the latest software available. The
following describes how to use an IBM compatible computer with
Hyper Terminal™ software (included with Windows® 95, 98, XP
or 2000 operating systems) to collect the RS232 data from your
Freeze Dryer:
1. Make sure that the Freeze Dryer is properly connected to the

communication port on the computer.
2. Open Hyper Terminal™ software.
i)Windows® 95 or 98 use:
START/PROGRAMS/ACCESSORIES.
ii) Windows® 2000 or XP use:

START/PROGRAMS/ACCESSORIES/COMMUNICATIONS
The first time Hyper Terminal™ is opened a dialogue box

requesting an area code and phone number will appear. Enter
the appropriate numbers and continue.
3. The “Connection Description” dialogue box will open. Type in

a user defined name and select an icon for the new connection.
Press “OK.”
4. The “Connect To” dialogue box will open. Using the down
arrow selection button, select the communication port to which
the cable has been connected. Press “OK.”
39
5. The “Com X Properties” dialogue box will open. Enter the

appropriate data properties and press “OK.”
40
6. When the Freeze Dryer main power switch is on, the data will
be transmitted and updated at the time intervals selected by the
user.
41
CHAPTER 7
TROUBLESHOOTING
Refer to the following if your Freeze Dryer fails to operate
properly. If the suggested corrective actions do not solve your
problem, contact Labconco for additional assistance.
Labconco Freeze Dry Systems that are clean, dry and without
samples attached should reach a vacuum of 0.133 mBar within 10
minutes and should achieve an ultimate vacuum of 0.033 mBar
within 18 hours when the refrigeration is operating. If the Freeze
Dryer does not obtain a satisfactory vacuum, perform the following
maintenance tests.
I. Vacuum Pump
First make sure that the vacuum pump operates. If it fails to
operate, check the electrical connections of the Freeze Dryer to the
power source and then check the electrical connection of the
vacuum pump to the Freeze Dryer. If the vacuum pump has a
power switch, make sure that it is turned on. If the vacuum is not
adequate when the vacuum pump is operating, proceed with the
following steps:
1. Check the oil and ensure it is clear and clean. If the oil
looks cloudy or has any particulates, replace the pump oil.
Sometimes it may be necessary to flush the pump with
clean oil several times. To flush the pump, run the pump 5
to 10 minutes to allow the oil to warm up. Drain the oil
and refill with clean oil. Repeat as necessary.
2. Check the oil level in the pump. Ensure it is filled to the
correct level.
3. Check vacuum hose connections from the pump to the
Freeze Dryer and try running the unit.
42
Chapter 7: Troubleshooting
If vacuum problems continue, consider obtaining a second vacuum

gauge capable of reading a vacuum of 0.010 mBar. It is often
useful in determining if the vacuum pump is operating properly
and the vacuum sensor reading is accurate.
4. Isolate the pump by disconnecting the vacuum hose from

the Freeze Dryer. Deadhead the pump by inserting the
vacuum sensor from a secondary vacuum gauge into the
end of the vacuum hose and observe the vacuum reading
obtained. Confirm that the pump is capable of achieving an
ultimate vacuum less than 0.010 mBar or approximately 10
microns. If an inadequate vacuum reading is obtained, the
pump has most likely failed and may need to be replaced or
rebuilt.
II. Gaskets, Tubing, Connections, Sample

Valves
1. Check all sample valves on the drying chamber/manifold
and ensure all valves are closed or in the vent position.
Check to ensure all fittings are tight and sealed properly
against the chamber. Inspect valves for cracks or cuts.
2. Inspect gasket(s) for cracks or defects. Ensure the gasket is
clean. Apply a thin coat of vacuum grease to the gasket.
Keep in mind too much vacuum grease can actually cause
leaks.
3. Check the drain line and ensure the drain plug is installed
and the tube appears to be in good condition.
4. Check all rubber vacuum tubing for signs of deterioration
or cracking.
5. Check all connections and make sure they are secure and
leak tight.
6. When checking the sample valves, pull as much vacuum as
possible. If a vacuum indication is displayed, wiggle or
rotate the valves and watch the gauge for any fluctuations.
Fluctuations can indicate a potential vacuum leak. If the
valve seems to be in good condition, remove the valve and
apply a thin coat of vacuum grease to the stem and the
outside sealing surface of the valve body, and reinstall the
valve. DO NOT APPLY VACUUM GREASE TO THE
SAMPLE VALVE GASKETS, WHICH SEAL TO THE
WALL OF THE DRYING CHAMBER. If the valve still
seems to be the source of the problem, remove the valve
and stopper the hole with a rubber stopper. Continue
checking the other valves.
43
7. Make sure that the sample valve bulkhead nuts are tight.
Either tighten by hand or use the wrench supplied with
chambers. To use the wrench, first remove the knob and
stem assembly and also the valve body. The pins on the
wrench fit into the round holes of the nut. The nut should
be snug, but avoid over-tightening. Replace the valve
body, knob and stem assembly.
The illustrations below show how the sample valve installs on

a chamber and a manifold.
Knob & Stem Valve Body

Assembly
Valve Assembly (Clear Chamber with Valves)
44
Manifold Assembly Valve Body Bulkhead Nut
Knob & Stem Valve Body Trim Ring Gasket

Knob & Stem Thrust Washer Bulkhead
Assembly (No grease
Assembly Fitting
required)
Valve Assembly (Manifold) Valve Assembly (Stainless Steel Chamber)
III. System Components and Collection

Chamber Isolation
1. Remove the drying chamber or manifold.
2. Leave the gasket on and turn a large freeze dry flask upside
down to cover the connection port.
3. Start the freeze dryer and observe the vacuum indication.
If the vacuum indication is good, then the problem is in the
drying chamber or manifold and you should return to
Section II, Gaskets, Tubing, Connections, Sample Valves.
45
Freeze Dry Flask
Gasket
The following test allows you to check the pump and the
connections from the pump to the vacuum tube.
1. Place a rubber stopper in the vacuum port in the left side of

the collector chamber and another in the drain port in the
bottom.
2. Restart the vacuum system and check your vacuum
indication. Insufficient vacuum indicates a bad pump or a
leak in the connections from the pump to the side of the
chamber.
Stopper Collector
Coil
46
The following test is used to check the collection chamber

integrity. The figure below points out potential areas to locate a
leak:
Collector
Chamber
Areas for
Potential Leaks
1. Remove the stopper from the side of the chamber and place
a freeze dry flask over the connection port.
2. Fill the collection chamber with approximately 2 inches of
water, enough to cover all fittings. Replace the collection
chamber lid and turn on the vacuum pump. Allow the
vacuum pump to run for approximately 5 to 10 seconds. (If
the vacuum pump is left on, the water will begin to boil and
the test will not be effective). Look inside the chamber for
any bubbling while the pump is running and after you shut
the pump off.
3. If bubbling is observed around the bulkhead fittings, access
the bottom of the chamber and remove the insulation.
Tighten the appropriate fitting by placing a wrench on the
fitting inside the chamber and use a second wrench to turn
the nut on the bottom of the chamber. Be careful not to
damage the evaporator coils or the brazed joints to the
refrigeration system. Once the fitting is tightened, perform
the test again. Should the bubbling still be present, loosen
the bulkhead fittings and apply vacuum grease to the O-
rings, then reassemble and test.
47
O Ring and
Vacuum Grease
Collector Coil
4. If bubbling was observed on the chamber surface, the

chamber must be replaced. This type of leak cannot be
successfully repaired. The leading cause of a chamber
surface leak is corrosive residue left in the chamber after
use.
Refrigeration Module Operation

Under a no-load condition, the FreeZone Single Stage Freeze Dry
System can achieve a collector temperature of –50°C or lower
when the system is under vacuum, within 40 minutes when the
vacuum pump is running, depending on ambient temperature and
humidity. Cascade Freeze Dry Systems will achieve –84°C within
40 minutes.
Cascade Systems (those that operate @ -84°) consist of two vapor-

compression refrigeration systems in series connected together via
a heat exchanger. Each system has a compressor, condenser,
capillary tube metering device and an evaporator. During
operation the evaporator of the “high stage” system refrigerates the
condenser of the “low stage” system. This takes place in the heat
exchanger. The low stage and high stage systems are balanced by
design, however, sometimes that balance can be disrupted during
operation and the unit will not function properly. If the unit is
overloaded, or if the unit is defrosted and restarted in a short time
interval, system unbalance is possible. If system unbalance occurs,
turn the Freeze Dryer off and allow the unit to soak at ambient
temperature for 2 to 4 hours.
If any repairs are required on the refrigeration module, contact

your local laboratory supply dealer. If your laboratory supply
dealer is unable to provide assistance, please call Labconco.
Repairs should only be undertaken by a competent refrigeration
technician or through an authorized Labconco service agency.
48
CHAPTER 8
MODIFYING YOUR
FREEZE DRYER
DISPLAY
Your Freeze Dryer has been carefully calibrated and tested before
shipping, however under certain circumstances it may be necessary
to adjust the calibration of the temperature and/or vacuum display
or to modify alarm points. Adjustments may be necessary if the
Freeze Dryer requires service or if it is operating on a line voltage
outside the voltage range at which the alarm was preset. This
DOES NOT mean that the Freeze Dryer may be operated at a
voltage outside the ranges shown in Appendix C.
Temperature and Vacuum Display

An offset may be added to the collector temperature or vacuum
display. Use an accurate traceable reference to compare the
readings.
Temperature offset may be varied ±5°C in 1°C increments.

Vacuum offset may be varied ±0.020 mBar in 0.001 mBar
increments.
Line Voltage Alarm Points

The Freeze Dryer is designed to alarm if the line voltage varies
more than ±10% from nominal line voltage. Models rated to
operate on 115V are preset to alarm if the voltage drops below
approximately 103V or rises above approximately 127V. Models
rated to operate on 230V will alarm if the voltage drops below
49
Chapter 8: Modifying Your Freeze Dryer Display
approximately 206V or rises above approximately 254V. Some

models are designed to operate below these ranges (see Appendix
C). In these cases it is permissible to lower the low voltage alarm
point to prevent nuisance alarms from occurring.
Low line limit may be lowered in 5 increments of
approximately 2 to 3V increments for 115V models or
disabled.
Low line limit may be lowered in 5 increments of
disabled.
High line limit may be raised in 5 increments of
disabled.
High line limit may be raised in 5 increments of
disabled.
Moisture Sensor Alarm

The moisture sensor alarm may be disabled. It is shipped enabled
as the factory default setting.
Modifying the Display
To enter an offset or to configure the alarms, perform the following
steps:
Press and hold MENU button (approximately 10 seconds)
until the display shows:
PRODUCTION MENU
MASTER RESET?
It is recommended that you do NOT perform a Master
Reset because all offsets and configurations that have been
entered will be lost. If you must perform a Master Reset,
hold SELECT approximately 5 seconds.
This will reset:
Vacuum units to mBar
Vacuum set point to 0 mBar
Temperature units to °C
Refrigeration total hours to 0
Vacuum pump total hours to 0
RS232 transmission rate to 10 seconds
Temperature offset to 0°C
Vacuum offset to 0 mBar
Low line voltage to 0 V offset
50
High line voltage to 0 V offset

Moisture sensor to enabled
Refrigeration to operate in Manual Mode
The display will default to the main freeze dry display information.
If you do not want to restore all factory settings, but want to adjust
offsets, press MENU briefly and the display will show:
COLLECTOR TEMP OFFSET:
OC
Press SELECT until the appropriate offset is shown. Each

number represents 1°C
Press MENU and, if the drying chamber has been installed, the
display will show:
SDC TEMP. OFFSET:
O C
Press SELECT until the appropriate offset is shown. Each number

represents 1°C.
Press MENU and the display will show:
VACUUM OFFSET:
O uBar
Press SELECT until the appropriate offset is shown. Each

number represents 0.001 mBar
Press MENU and the display will show

LOW LINE OFFSET:
0
Press SELECT until the appropriate offset is shown. If the

Freeze Dryer is operating on nominal 115V, each number
represents 2V. If 3 is entered into the display, the low line
alarm will alarm when the voltage drops to approximately
97V, for example. 103-(2x3)=97V. If the Freeze Dryer is
operating on nominal 230V each number represents 4V (if
3 is entered into the display, the low line alarm will alarm
when the voltage drops to approximately 194V, for
example. 206-(4x3)=194V.
There will be no alarm indicated if DISABLED is selected.
51

HIGH LINE OFFSET:
0
Press SELECT until the appropriate offset is shown. If the

Freeze Dryer is operating on nominal 115V, each number
represents 2V. If 3 is entered into the display, the high line
alarm will alarm when the voltage raises to approximately
133V, for example. 127+(2x3)=133V. If the Freeze Dryer
is operating on nominal 230V each number represents 4V
(if 3 is entered into the display, the low line alarm will
alarm when the voltage drops to approximately 266V, for
example. 254+(4x3)=266V. There will be no alarm
indicated if DISABLED is selected.

DRYING CHAMBER:
NOT INSTALLED
Press and hold SELECT to change the status.
Press MENU and the display will show:

PURGE VALVE:
NOT INSTALLED

DEFROST HEATER:
NOT INSTALLED

MOISTURE SENSOR:
INSTALLED
Press and hold SELECT if you want to disable the moisture
sensor.
Press MENU and the display again show

SHELL FREEZER:
NOT INSTALLED
52

HOLD SELECT TO CLEAR
ALL TOTAL HOURS?
If you want to reset Total Hours, press and hold SELECT until an
audible beep is heard. The display will default to the main freeze
dry display information.
If you do not want to set Total Hours, press MENU and the display
will show.
PRODUCTION MENU:
MASTER RESET?
The routine will repeat by pressing MENU or want approximately

10 seconds for the display to default to the main freeze dry
information display information.
In order to store offsets in memory, you Must Press and Hold

MENU until the display shows.
PASSWORD:
Wait approximately 10 seconds and the display will default to the

main freeze dry display information. This can be done anytime
throughout the Modifying the Display routine.
53
APPENDIX A
FREEZE DRYER
COMPONENTS
The following pages list components that are available for your
Freeze Dryer. The parts shown are the most common replacement
parts. If other parts are required, contact Product Service.
54
Appendix A: Freeze Dryer Components
Item Model Part No. Description

1. All 7689900 Lid Gasket – Collector
2. All 7532900 Lid Collector
3. All 7408400 Lid Gasket - Drying Chamber-Shell Freezer
4. All 7408300 Lid - Drying Chamber
6L 7403100 Lid -Shell Freezer
5 6L 7750602 Compressor 115V, 60 Hz.
6L 7750601 Compressor 230V, 50 Hz.
6L Cascade 7591800 Compressor 115V, 60 Hz. Hi Stage
6L Cascade 7591800 Compressor 115V, 60 Hz Lo Stage
6L Cascade 7591801 Compressor 230V, 50 Hz. Lo Stage
12L 7592000 Compressor 230V, 60 Hz
18L 7391800 Compressor 239V, 60 Hz
6. 6L 7591800 Compressor 115V, 60 Hz. Shell Freezer
6L 7591801 Compressor 230V, 50 Hz. Shell Freezer
6L 7591802 Compressor 230V, 60 Hz. Shell Freezer
7. 6L 7953800 Motor Fan 115V
All 7953801 Motor Fan 230V
8. All 1302300 Switch
9. All 7403500 Label Control Panel
All 7403501 Label Control Panel with Purge
All 7403502 Label Control Panel with Purge and Shell Freezer/Drying Chamber
10. All 7445500 Printed Circuit Board Control
11. All 7448000 Printed Circuit Board RS232
12. All 7728000 Drain Plug
13. All 1643600 O Ring
14. All 7645904 Drain Hose
15. All 7646000 Vacuum Hose (Not Shown)
16. 6L 1336400 Power Cord 115V
All 1342100 Power Cord 230V
17. All 7445400 Vacuum Sensor
18. All 7515300 Temperature Sensor – Collector (Not Shown)
19. 6L 7515300 Temperature Sensor – Shell Freezer (Not Shown)
55
Item Model Part No. Description

20. All 7515300 Temperature Sensor – Drying Chamber (Not Shown)
21. 6L, 12L, 18L 7404900 Wire Harness (Not Shown)
6L, 12L Cascade 7446500 Wire Harness (Not Shown)
22. All 7514900 Wire Harness Control (Not Shown)
23. All 7418300 Wire Harness RS232 (Not Shown)
24. All 7432700 Valve Vacuum Bleed
25. 6L 1363102 Valve Purge 115V
All 1363103 Valve Purge 230V
26. All 7814600 Valve Drying Chamber
27. 6L 7407300 Heater Drying Chamber 115V
All 7407301 Heater Drying Chamber 230V
28. All 7429700 Moisture Sensor
29. 6L 1289200 Relay Vacuum Pump 115V
All 1289100 Relay Vacuum Pump 230V
30. All 1289200 Relay Refrigeration
31. All 7403800 Filter Vacuum Bleed Valve
56
57
58
APPENDIX B
FREEZE DRYER
DIMENSIONS
59
APPENDIX C
FREEZE DRYER
SPECIFICATIONS
This Appendix contains technical information about the Freeze
Dryer including electrical specifications, environmental operating
conditions and wiring diagrams.
Electrical Specifications, 6L, 12L, and 18L Console

Voltage Amperage
w/o Max with
Catalog Operating Vacuum Vacuum
Number Description Nominal Range Frequency Phase Pump Pump
7753020 6 Liter Freeze Dryer 115 103-127 60 1 9 16

100 90-110 50 1 9 16
100 90-110 50 1 9 16
100 90-110 50 1 9 16
100 90-110 50 1 9 16
100 90-110 50 1 9 16
100 90-110 50 1 9 16
60
Appendix C : Freeze Dryer Specifications
Voltage Amperage
w/o Max with
Catalog Operating Vacuum Vacuum
Number Description Nominal Range Frequency Phase Pump Pump

100 90-110 50 1 13 16
100 90-110 50 1 13 16
7753532 6 Liter Freeze Dryer 230 198-254 50 1 5.5 10
7934020 6 Liter Cascade Freeze Dryer 115 103-127 60 1 11 16

100 90-110 50 1 11 16
100 90-110 50 1 11 16
100 90-110 50 1 11 16
100 90-110 50 1 11 16
100 90-110 50 1 11 16
100 90-110 50 1 11 16
7934030 6 Liter Cascade Freeze Dryer 230 198-254 50 1 5.5 10
61
Appendix C: Freeze Dryer Specifications
Voltage Amperage
w/o
Catalog Operating Vacuum Max with
Number Description Nominal Range Frequency Phase Pump Vacuum Pump


62
Environmental Conditions
• Indoor use only.

• Maximum altitude: 6562 feet (2000 meters).
• Ambient temperature range: 41° to 104°F (5° to 40°C).
• Maximum relative humidity: 80% for temperatures up to
88°F (31°C), decreasing linearly to 50% relative humidity
at 104°F (40°C).
• Main supply voltage fluctuations not to exceed ±10% of the
nominal voltage.
• Transient over voltages according to Installation Categories
II (Over voltage Categories per IEC 1010). Temporary
voltage spikes on the AC input line that may be as high as
1500V for 115V models and 2500V for 230V models are
allowed.
• Used in an environment of Pollution degrees 2 (i.e., where
normally only non-conductive atmospheres are present).
Occasionally, however, a temporary conductivity caused by
condensation must be expected, in accordance with IEC
664.
63
Wiring Diagram Catalog #77530xx and 77535xx, 79340xx (115V, 60 Hz

Models)
64
Wiring Diagram Catalog #79340xx, (230V, 50 or 60 Hz

Models)
65
Wiring Diagram Catalog #77530xx, 77535xx, 77540xx, 79600xx and

77550xx (230V, 50 or 60 Hz Models)
66
APPENDIX D
FREEZE DRYER
ACCESSORIES
The following accessories are available for the Freeze Dryer.
PART # DESCRIPTION
1467700 Vacuum Pump
Two stage direct drive pump, 195 liters/minute. 115 VAC,
50/60 Hz, single phase, 7.8 amps. Includes Pump Exhaust Filter
1473400. (Catalog #1473400)
7739403 Vacuum Pump

50/60 Hz, single phase, 4.0 amps. Includes Pump Exhaust Filter
1473400. (Catalog #1473400)
7439000 Vacuum Pump

50/60 Hz, single phase 5.8 amps. Includes Pump Exhaust Filter.
(Catalog #7670400)
7439200 Vacuum Pump

(Catalog #7670400)
7769600 Vacuum Pump, Chemical Resistant

(Catalog #7670400)
7769800 Vacuum Pump, Chemical Resistant

50/60 Hz, single phase 2.9 amps. Includes Pump Exhaust
Filter.(Catalog #7670400)
67
Appendix D : Freeze Dryer Accessories
PART # DESCRIPTION
1472200 Pump Inlet Filter
Disposable filter that prevents oil back streaming and protects vacuum
pump from sub micron particles. Fits vacuum pumps 1466700 and
7739403.
1473400 Pump Exhaust Filter

Disposable filter that removes visible oil mist and odor from vacuum
pump exhaust. Fits vacuum pumps 1467700 and 7739403.
1473200 Replacement Element, Oil Mist, Pump Exhaust Filter

Fits pump exhaust filter 1473400.
1473300 Replacement Element, Odor, Pump Exhaust Filter,

package of 5
Fits pump exhaust filter 1473400 or vacuum pumps 1467700 and
7739403.
7670400 Replacement Filter – Element

Disposable filter that removes oil mist from the vacuum pump exhaust.
Fits vacuum pumps 7439000, 7439200, 7769600 and 7769800
1988000 Vacuum Pump Oil, 1 Liter

A molecularly distilled hydrocarbon oil with low vapor pressure.
For vacuum pumps 1467700 and 7739403
7772000 Soda Acid Trap

Secondary trap that prevents migration of corrosive chemicals into
vacuum pump.
7772100 Replacement Media for Soda Acid Trap
7772700 Vacuum Pump Oil 1 Liter

A mineral oil with low vapor pressure.
For vacuum pumps 7439000, 7439200, 7769600, 7769800
7772500 Carbon Solvent Trap

Secondary trap that prevents migration of organic solvents into vacuum
pump.
7772600 Replacement Activated Carbon Media for Carbon Solvent Trap
68
PART # DESCRIPTION
7538000 Secondary Vacuum Cold Trap
Provides additional protection for the vacuum pump when
processing low eutectic samples.
9 ¾" high x 7 7/8" diameter, 304 stainless steel with ¾" vacuum
connections. For use with dry ice and solvent. Cools to
approximately –75°C.
7522800 12 Port Drying Chamber

9 ¾" high x 7 7/8" diameter, 304 stainless steel with 12 freeze dry
valves.
7522900 16 Port Drying Chamber
13" high x 138" diameter, 304 stainless steel with 16 freeze dry
valves.
7443500 Clear Drying Chamber with 8 Valves
For bulk drying or drying in flasks. 9.0 Dia.
7444000 Clear Drying Chamber with 8 Valves
For bulk drying or drying in flasks. 12.0 Dia.
7442900 Clearing Drying Chamber
For bulk drying. 9.0 Dia.
7867000 Clear Drying Chamber
For Bulk Drying 12.0 Dia.
7521000 Heated Drying Chamber
10 ½" high x 9" diameter type 304 stainless steel. The 3 shelf
product heaters heat to 43°C (110°F). 115V.
7521001 Heated Drying Chamber
10 ½" high x 9" diameter type 304 stainless steel. The 3 shelf
product heaters heat to 43°C (110°F). 230V.
7509200 Product Heater
For use in chamber 7522800. Provides 3 heated shelves operating
at 43°C (110°F). 115V
For use in chamber 7522800. Provides 3 heated shelves operating
at 43°C (110°F). 230V
7442100 Drying Rack- Unheated
Provides three shelves. For use in chambers 7443500 and
7522800.
7441700 Drying Rack – Unheated
Provides three shelves for use in chambers 7444000, 7867000,
7522900
7522300 20 Port Manifold
10" high x 27 ½" wide x 8 5/8" deep. Type 304 stainless steel
manifold with 20 freeze dry valves.
69
PART # DESCRIPTION
7522400 10 Port Manifold with support shelf
10" high x 26" wide x 6-5/8" deep. Type 304
Stainless Steel Manifold with 10 Freeze Dry Valves
& 1 Shelf
7522500 20 Port Manifold with support shelves
10" high x 26" wide x 9-1/2" deep. Type 304
Stainless Steel Manifold with 20 Freeze Dry valves
and 2 shelves.
7868500 48 Port Ampule Manifold
28 5/8" high x 5" wide x 5" deep. Type 304
stainless steel with
48 each ¼" tube stems.
7509600 Sample Valve Kit
Includes neoprene valve body, knob and installation
parts.
7439902 Glass Collector Chamber Lid
For use with solvlents that attack the acrylic lid.
7439902 Glass Collector Chamber Lid
For use with solvlents that attack the acrylic lid.
For use in chamber 7522900, 7444000 and
7867000. Provides 3 heated shelves operating at
43°C (110°F). 115V
7867000. Provides 3 heated shelves operating at
43°C (110°F). 230V
7509400 Product Heater with Variable Heat
7867000. Provides variable heat up to 43°C
(110°F). 115V
7509401 Product Heater with Variable Heat
For use in chamber 7522900, 7444000 and 7867000
7806020 Bulk Tray Dryer
115V, 60 Hz, three shelves, 630 square inches of
area, provides heat control
area, provides heat control with 6 port manifold
area, provides heat control with RS232 output
connection.
70
PART # DESCRIPTION
115V, 60 Hz, three shelves, 630 square inches of area, provides heat
control with 6 port manifold and RS232 output connection.
230V, 50/60 Hz, Three shelves, 630 square inches of area, provides
heat control.
heat control. With 6 port manifold.
heat control. With RS232 output connection.
heat control. With 6 port manifold and RS232 output connection.
7948020 Stoppering Tray Dryer
115V, 60 Hz, three shelves, 600 square inches of area, provides
temperature control and stoppering under vacuum.
7726500 6 Port Manifold for use with Stoppering Tray Dryer
Mounts between the Stoppering Tray Dryer and the base unit and
provides 6 freeze dry valves.
7537800 Cable
Connect the RS232 output from the Freeze Dryer (or Freeze
Dryer/Tray Dryer combination) to an IBM compatible computer with a
9-pin serial data port.
7537801 Cable
Connects the RS232 output from the Freeze Dryer (or Freeze
Dryer/Tray Dryer combination) to an IBM compatible computer with a
25-pin serial data port.
7761500 Isolation Valve
Mounts between the Stoppering Tray Dryer and the base unit which
provides a way to isolate the base unit vacuum system from the
Stoppering Tray Dryer vacuum system.
7390702 6L Baffle
Mounts in the collector chamber to increase ice holding capacity when
operating with vacuum control.
7390701 12L Baffle
Mounts in the collector chamber to increase ice holding capacity when
operating with vacuum control.
71
Appendix D: Freeze Dryer Accessories
Fast-Freeze® Flasks
Variety of adapters Compatible with
available. You may all major brands of
select from glass or laboratory freeze dry
stainless steel apparatus.
adapters, available
straight or with 45° No complex filter
bend. (Required — retainer is necessary.
order separately.) For those who use
filters, they are easily
Top seals easily. The inserted between the
flexible silicone rubber adapter and top of
top snaps on and off the flask. One hun-
easily, yet provides a dred filters are sup-
reliable, high vacuum plied with each flask.
seal.
Only two pieces

per flask. Wide mouth
The complete opening loads fast,
Fast-Freeze Flask cleans easily.
has only two
components:
• a high strength Horizontal shell
borosilicate freezing. Flask
glass bottom may be placed in
to withstand a horizontal posi-
extreme tion and rotated
temperatures in a bath for shell
Fast-Freeze Flasks are specially designed to be easier to and high freezing.
vacuum.
handle, faster to load and more convenient to use than other
freeze dry glassware now in your laboratory. Compatible • a flexible, non-
contaminating
silicone rubber Available in nine
with all major brands of laboratory freeze dry equipment, convenient sizes.
top.
Fast-Freeze Flasks eliminate the risk of contamination from No vacuum
vacuum grease, reduce spillage of valuable samples and grease is
require no washers, gaskets or retainers. necessary. Flat bottom
No threads, reduces spills,
hooks or springs provides better
How to select Fast-Freeze Flasks for are needed. balance.
your Freeze Dry System Entire flask may
be autoclaved.
Select Fast-Freeze Flasks based on your sample sizes. Flasks
should be filled no more than one-third of their volume so
that maximum surface area is achieved and efficient Adapters
lyophilization is assured. A complete Fast-Freeze Flask Add the Adapters for connecting
includes a rubber top, glass bottom and a supply of filter the Fast-Freeze Flasks to the valve
paper. Tops, bottoms and filter paper are available separate- ports on your drying chamber or
ly as replacement components. Adapters are required to manifold. Choose borosilicate glass
attach flasks to freeze dry valve ports. or stainless steel adapters in 1/2"
and 3/4" diameters.
Flask Complete Flask Flask Flask Top Dimensions/
Size Flask Bottom Top Adapter Flask Bottom Diameter Straight 45° Bend
Diameter* HxD Adapter Adapter
40 ml 7540000 7542000 7544000 1/2" 76 mm x 34 mm Borosilicate Glass
80 ml 7540200 7542200 7544000 1/2" 115 mm x 34 mm 1/2" flask top to 1/2" valve* 7545000 7545600
120 ml 7540300 7542300 75442-00 3/4" 68 mm x 59.2 mm 3/4" flask top to 3/4" valve* 7545200 7545800
150 ml 7540400 7542400 7544200 3/4" 85 mm x 59.2 mm 1/2" flask top to 3/4" valve* 7545400 7546000
600 ml 7540800 7542800 7544400 3/4" 135 mm x 90.2 mm Stainless Steel
2000 ml 7541200 7543200 7544400 3/4" 380 mm x 90.2 mm
7544810 Replacement Filter Paper
*Valves on the freeze dry systems, drying chambers and manifolds offered in this catalog fit adapters
of both 1/2” and 3/4" sizes. Size information is provided for selecting adapters for older Labconco mod- 1000 (10 packages of 100). 1" diameter (28mm). Pore size 17 microns.
els and other freeze dryers. Shipping weight 0.5 lb.
72
Lyph-Lock® Flasks
Borosilicate glass Compatible with
adapters with all major
either 19/38 or 24/40 brands of labo-
standard taper joints ratory freeze
have 90° bend. dry apparatus.
(Required — order
separately.)
Only three pieces

per flask — no
hooks or springs. Silicone rubber
The complete seal grasps top
Lyph-Lock Flask and bottom.
includes: The flexible ring
• a flask top of holds securely
high strength together during
borosilicate pre-freezing
glass and lyophiliza-
• a flexible, non- tion.
contaminating
silicone rubber
seal
• a flask bottom
of borosilicate
glass to with-
stand extreme
temperatures
and high
Lyph-Lock Flasks simplify your lyophilization procedures vacuum.
because they have only three pieces per flask — a high
strength borosilicate glass top and bottom with a silicone Available
in seven
rubber ring seal. The unique wide-mouth design helps you convenient sizes. Flat bottom
load samples easily and lyophilize efficiently. reduces spills,
Entire flask may provides better
be autoclaved. balance.
How to select Lyph-Lock Flasks for
your Freeze Dry System Provides a high
vacuum seal for
Select the Lyph-Lock Flasks based on your sample sizes. efficient
lyophilization.
Flasks should be filled to no more than one-third of their
volume so that maximum surface area is achieved and effi-
cient lyophilization is ensured. A complete Lyph-Lock Flask
includes a glass top and bottom and a rubber ring seal. Tops,
bottoms and seals are available separately as replacement Adapters
components. Adapters are required to attach flasks to freeze Add the Adapters for connecting the Lyph-Lock Flasks to the
dry valve ports. valve ports on your drying chamber or manifold.
Flask Complete Complete Flask Flask Lyph-Lock Flask Dimensions 90° Bend Description
Size Flask Flask Top Top Seal Bottom Flask Bottom Adapter
19/38 STJ 24/40 STJ 19/38 STJ 20/40 STJ H x ID
7568000 Connects 19/38 STJ Flask Top to 1/2" valve*
25 ml 7550000 7554000 7552000 7556000 75590-00 75570-00 37 mm x 34 mm
50 ml 7550200 7554200 7552000 7556000 7559000 7557200 67 mm x 34 mm 7568200 Connects 19/38 STJ Flask Top to 3/4" valve*
100 ml 7550400 7554400 7552200 7556200 7559200 7557400 50 mm x 59.2 mm 7568400 Connects 24/40 STJ Flask Top to 1/2" valve*
250 ml 7550600 7554600 7552200 7556200 7559200 7557600 110 mm x 59.2 mm
7568600 Connects 24/40 STJ Flask Top to 3/4" valve*
500 ml 7550800 7554800 7552400 7556400 7559400 7557800 103 mm x 90.2 mm
750 ml 7550900 7554900 7552400 7556400 7559400 7557900 145 mm x 90.2 mm *Valves on the freeze dry systems, drying chambers and manifolds offered in this catalog fit adapters
of both 1/2” and 3/4" sizes. Size information is provided for selecting adapters for older Labconco
1000 ml 7551000 7555000 7552400 7556400 7559400 7558000 187 mm x 90.2 mm models and other freeze dryers.
Serum Bottles and Vials

Threaded Vials
Stoppers and Threaded Vials with Screw Caps are supplied
in packages of 200.
Size Vials with Stoppers

Screw Caps
5 ml 7762300 7762200
10 ml 7762600 7762200
Accessories
Perfect for long term storage of freeze dried samples.

Labconco Serum Bottles and Threaded Vials are specifically
designed for lyophilization applications. Their uniform thin
wall construction ensures even freezing and drying. Bottles
and vials are ideal containers for use in the FreeZone
Stoppering Tray Dryer. Serum bottles also connect to valve Seal Crimper
ports on drying chambers and manifolds. Secures tear-away Aluminum Seals.
Serum Bottles 7578000 Seal Crimper for 13 mm corkage.
Serum Bottles, Stoppers and Seals are supplied in pack- Shipping weight 3 lbs. (1.4 kg).
ages of 100. 7578100 Seal Crimper for 20 mm corkage.
Shipping weight 3 lbs. (1.4 kg).
Vacuum Stoppering Adapter

7593000 Adapter connects to valve ports for manual stop-
pering of 20 mm corkage serum bottles under original vacu-
um. The stopper and serum bottle are inserted into the
adapter body and lyophilization begins. After the process is
completed, the researcher slides the stopper into position
so when the valve is turned from vacuum to vent the serum
bottle is tightly sealed by the stopper. The ejector tube is
then used to force the serum bottle out of the adapter.
Size 20 mm 13 mm Split Aluminum Sleeve-Type Shipping weight 1 lb. (0.4 kg).
Corkage Corkage Stoppers Seals Stoppers
2 ml 7575010 7576010 7577010 Stoppering Adapter Body Serum Bottle
3 ml 7575210 7576010 7577010
5 ml 7573010 7576210 7577110 7577510 Valve Port
10 ml 7573210 7576210 7577110 7577510
20 ml 7573410 7576210 7577110 7577510
30 ml 7573610 7576210 7577110 7577510
50 ml 7573810 7576210 7577110 7577510
100 ml 7574010 7576210 7577110 7577510
125 ml 7574210 7576210 7577110 7577510 Vent Hole
Ejector Tube Stopper
74
Ampules
Accessories
Oxygen/Natural Gas Sealing Torch

7578500 Torch specifically designed for flame sealing freeze
dry ampules. Seals all types of heat-resistant glass. Connects
to natural gas, butane or propane and oxygen with 1/4" ID
hose connectors. Shipping weight 3 lbs. (1.4 kg).
Labconco Ampules are fabricated of highest quality borosili-

cate glass for strength and durability. They are available in
five different configurations to provide the ideal ampule for
your specific lyophilization requirements, from tray drying to
flame sealing applications. Ampule Valve Adapters
7593401 Adapter connects ampules to valve ports or stainless
Ampules
steel stems. Ten per package. Shipping weight 0.5 lb. (0.2 kg).
Ampules are supplied in packages of 100.
Stoppers
7572510 Stopper for Stoppering Ampules 75723-10.
100 per package. Shipping weight 3 lbs. (1.4 kg).
Size Straight Bulb-Type Pre-Scored Round Stoppering

Flat Bottom Bottom
1 ml 7572710 7570010 7570610
2 ml 7570810 7572310
Trident Adapter
4 ml 7572810
7762700 Three Way Adapter permits attachment of three
5 ml 7570210 7571010
ampules to a single valve port. Ampules are attached using
10 ml 7571210 7571610 Ampule Valve Adapters or 1/8" surgical tubing (not provided).
25 ml 7571810 Cavity in adapter body can be filled with cotton fiber media
50 ml 7572010 to help prevent contamination between samples.
Shipping weight 3 oz. (0.1 kg).
76
For more information, please contact us:
ExpotechUSA
10700 Rockley Road
Houston, Texas 77099
USA
281-496-0900 [voice]
281-496-0400 [fax]
E-mail: sales@expotechusa.com
Website: www.ExpotechUSA.com

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User’s Manual

FreeZone® 6, 12 and 18 Liter

Part #7403400 Rev C

CHAPTER 3: GETTING STARTED 9

CHAPTER 4: USING YOUR FREEZE DRYER 18

CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 35

CHAPTER 6: USING THE RS232 RECEPTACLE 37

CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY 49

APPENDIX A: FREEZE DRYER COMPONENTS 54

APPENDIX B: FREEZE DRYER DIMENSIONS 59

APPENDIX C: FREEZE DRYER SPECIFICATIONS 60

APPENDIX D: FREEZE DRYER ACCESSORIES 67

Freeze Dry Process

Freeze drying is a process whereby water or other solvent is

Freeze Dry Rates

Up to the point of overloading the system, the greater the surface

The surface area and thickness of the sample can usually be

In order for lyophilization to occur, ice must be removed from the

The rate of freeze drying is directly proportional to the vapor

Freeze Dry Capacity

pressure and ultimately overloads the collector and vacuum pump.

If there is a problem with a particular type of sample melting when

Samples Containing Volatile

About This Manual

Chapter 1: Introduction provides a brief overview of the Freeze

Chapter 2: Prerequisites explains what you need to do to prepare

Chapter 3: Getting Started contains the information you need to

Chapter 4: Using Your Freeze Dryer discusses the basic operation

Chapter 5: Maintaining Your Freeze Dryer explains how to

Chapter 6: Using the RS232 Receptacle describes how to connect

Chapter 7: Troubleshooting contains a table of problems you may

Chapter 8: Modifying Your Freeze Dryer Display describes how

Appendix A: Freeze Dryer Components contains labeled diagrams

Appendix B: Freeze Dryer Dimensions contains comprehensive

Appendix C: Freeze Dryer Specifications contains product

Appendix D: Freeze Dryer Accessories lists the part numbers and

Carefully read this chapter to learn:

• the electrical supply requirements.

Refer to Appendix C: Freeze Dryer Specifications for complete

Refer to Appendix C: Freeze Dryer Specifications for dimensional

Vacuum Pump Requirements

Vacuum pumps used with 115V models should be equipped with

• unpack and move your Freeze Dryer.

The FreeZone Freeze Dry System may weigh as

Unpacking Your Freeze Dryer

IF YOUR FREEZE DRYER WAS DAMAGED IN

Freeze Dryer Components

Catalog Numbers 6, 12 and 18 Liter Console Models

7753020 6 Liter Freeze Dryer 115 60

7753522 6 Liter Freeze Dryer 115 60 x x

Catalog Numbers 6, 12 and 18 Liter Console Models

7754030 12 Liter Freeze Dryer 230 50

7960030 12 Liter Cascade Freeze Dryer 230 50

Catalog Numbers 6, 12 and 18 Liter Console Models

Plus the Following:

Setting Up Your Freeze Dryer

Vacuum Pump Connection

Make certain that the oil in the vacuum pump is

Optional Purge Valve

Drying Chamber or Drying Manifold

Chemical Resistance of Freeze Dryer

Acids Buffers Solvents

Methyl t-Butyl Ether (BTBE)